反应详情

NCS (0.826 g) was added portionwise to a solution of tert-butyldimethyl(2-(thiophen-2-yl)ethoxy)silane [WO 2008096129] (1.5 g) in chloroform (50 mL) and the resulting mixture was heated at reflux for 3 days. The mixture was diluted with DCM (100 mL) and washed with saturated aqueous sodium bicarbonate (2×100 mL) and brine (100 mL), then dried over sodium sulphate, filtered and evaporated. The residue was purified by silica gel chromatography eluting with isohexane to give the subtitled compound as a clear oil. Yield 1.00 g.

1. temperaturethe resulting mixture was heated
2. temperatureat reflux for 3 days
3. washwashed with saturated aqueous sodium bicarbonate (2×100 mL) and brine (100 mL)
4. dry with materialdried over sodium sulphate
5. filtrationfiltered
6. customevaporated
7. customThe residue was purified by silica gel chromatography
8. washeluting with isohexane